SPE-HPLC测定金鸡颗粒中3种生物碱含量

目的建立固相萃取-高效液相色谱法（SPE-HPLC）测定金鸡颗粒中盐酸药根碱、盐酸巴马汀和盐酸小檗碱3种生物碱含量的方法。方法选用WCX弱阳离子交换固相萃取小柱净化,采用Hvydro-RP 80A C18柱（250 mm×4.6 mm,5μm）,乙睛-0.05 mol/L磷酸二氢钠溶液（磷酸调pH 2.8,27∶73）为流动相,柱温为35℃,流速1.0 mL/min,检测波长为265 nm。结果盐酸药根碱、盐酸巴马汀、盐酸小檗碱分别在4.94～49.44 ng（r=1.000 0）、4.36～43.60 ng（r=0.999 9）、3.99～39.94 ng（r=0.999 9）范围内线性关系良好,加样回收率分别为97.63%（RSD=1.6%）、99.95%（RSD=3.1%）、99.01%（RSD=2.2%）。结论本方法操作简便,准确性、重复性好,可用于金鸡颗粒中盐酸小檗碱、盐酸巴马汀和盐酸药根碱的含量测定。

Determination of Three Alkaloids in Jinji Granules by SPE-HPLC

Objective To establish a solid-phase extraction with high-performance liquid chromatography（SPE-HPLC） method for the determination of jatrorrhizine hydrochloride,palmatine hydrochloride and berberine hydrochloride in Jinji Granules.Methods WCX weak cation SPE column was used to clean.The Hvydro-RP 80A C18 column（250 mm×4.6 mm,5 μm） was used at 35 ℃ with acetonitrile-0.05 mol/L sodium dihydrogen phosphoric acid（pH 2.8,27∶73） as the mobile phase,1.0 mL/min as the flow rate,265 nm as the detective wave length.Results The linear range were 4.94-49.44 ng（r=1.000 0） for jatrorrhizine hydrochloride,4.36-43.60 ng（r=0.999 9） for palmatine hydrochloride and 3.99-39.94 ng（r=0.999 9） for berberine hydrochloride.The average recovery was 97.63%（RSD=1.6%）,99.95%（RSD=3.1%） and 99.01%（RSD=2.2%）,respectively.Conclusions This method is simple,accurate and repeatable.It can be used for the determination of jatrorrhizine hydrochloride,palmatine hydrochloride and berberine hydrochloride in Jinji Granules.